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Dichloromethane → HCID 178519271, 화합물

HRID 259589
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HRID 259589 반응식
[C-:1]1([C:6]([CH2:8][CH2:9][CH2:10][CH2:11][C:12](Cl)=[O:13])=O)[CH:5]=[CH:4][CH:3]=[CH:2]1.[CH-:15]1[CH:19]=[CH:18][CH:17]=[CH:16]1.[Fe+2:20].[Cl-].[Al+3].[Cl-].[Cl-].[CH2:25](Cl)Cl>C1C=CC=CC=1>[C:12]([C:11]1[CH2:10][CH2:9][CH2:8][C:6]=1[C-:1]1[CH:5]=[CH:4][CH:3]=[CH:2]1)(=[O:13])[C:16]1[CH:17]=[CH:18][CH:19]=[CH:15][CH:25]=1.[CH-:1]1[CH:5]=[CH:4][CH:3]=[CH:2]1.[Fe+2:20]
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

5

반응물 3

HCID 6344DichloromethaneHCID 6451240Aluminum(III) ChlorideHCID 178521142HCID 178521142, 화합물

생성물 1

HCID 178519271HCID 178519271, 화합물수율 9%

시약·촉매·용매 1

HCID 241Benzene용매

실험 절차

Ferrocenoylvaleryl chloride (prepared as above and assumed to be 0.01 mole) was diluted with methylene chloride (10 mls.) and benzene (20 mls.) and the solution was cooled to 0°-5°. Aluminum chloride (2.6g; 0.02 mole) was then added with stirring over 30 minutes. After further stirring at room temperature for 2 hours, ice was added to the reaction mixture. The organic layer was then separated and washed successively with water, aqueous sodium bicarbonate solution, and water, before being dried over sodium sulphate. Evaporation under reduced pressure produced a brown oil from which chromatography on silica gel with toluene/ethyl acetate provided a pure sample of the required compound (0.32g; 9% yield) mp 135°-137°.

후처리

  1. temperaturethe solution was cooled to 0°-5°
  2. stirringAfter further stirring at room temperature for 2 hours
  3. additionice was added to the reaction mixture
  4. customThe organic layer was then separated
  5. washwashed successively with water, aqueous sodium bicarbonate solution, and water
  6. dry with materialbefore being dried over sodium sulphate
  7. customEvaporation under reduced pressure
  8. customproduced a brown oil from which chromatography on silica gel with toluene/ethyl acetate

출처 및 근거

ORD 기록
ord-e60386c63d844c85af62edccf68a9362
출처 데이터셋
uspto-grants-1977_07
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US04038413

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